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Solvent-free preparation method of 1, 4-DMCD

A technology of dimethyl cyclohexanedicarboxylate and dimethyl phthalate, which is applied in the field of catalytic hydrogenation preparation 1, can solve the problems of cumbersome treatment process, low yield, increased cost of solvent recovery, etc., and achieve optimized process, cost reduction effect

Inactive Publication Date: 2012-11-28
江苏恒祥化学股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The solvent is one of water or C1-C4 fatty alcohol or other solvents. The post-treatment process of DMCD prepared by this process is cumbersome, the yield is low, and the cost of solvent recovery is greatly increased.

Method used

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  • Solvent-free preparation method of 1, 4-DMCD

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Put 2t of DMCD into the mixing tank, add 0.9t of DMT, heat and stir, after it is completely dissolved, feed the material to the fixed bed of the first hydrogenation reaction at a flow rate of 200kg / h through a metering pump, control the temperature at 140°C, and the pressure at 4.0MPa , The detection reaction conversion rate was 99.7%, and the selectivity was 99.5%.

Embodiment 2

[0012] Put 2t of DMCD into the mixing tank, add 0.9t of DMT, heat and stir, after it is completely dissolved, feed the material to the fixed bed of the first hydrogenation reaction at a flow rate of 250kg / h through a metering pump, control the temperature at 140°C, and the pressure at 4.0MPa , The detection reaction conversion rate was 99.4%, and the selectivity was 99.2%.

Embodiment 3

[0014] Put 2t of DMCD into the mixing tank, add 0.9t of DMT, heat and stir, after being completely dissolved, feed the material to the fixed bed of the first hydrogenation reaction at a flow rate of 300kg / h through a metering pump, control the temperature at 140°C, and the pressure at 4.0MPa , The detection reaction conversion rate was 99.0%, and the selectivity was 98.8%.

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Abstract

The invention provides a solvent-free preparation method of 1, 4-DMCD. The common synthesis method of the 1, 4-CHDA dimethyl carbonate takes dimethyl terephthalate as a raw material, and takes one of water or C1-C4 fatty alcohol as a solvent, while, the solvent-free preparation method takes dimethyl terephthalate as the raw material, and directly takes 1, 4-DMCD as the solvent, so that the aftertreatment process can be eliminated, the obtained product can be directly used for the downstream product, the technology can be optimized, and the cost can be greatly reduced.

Description

technical field [0001] The invention relates to the preparation of 1,4-cyclohexanedicarboxylate by catalytic hydrogenation. Background technique [0002] Dimethyl 1,4-cyclohexanedicarboxylate (DMCD) is an intermediate monomer for the production of 1,4-cyclohexanedimethanol (CHDM). CHDM is used as a raw material for synthetic fibers or synthetic resins, especially for Modified materials used as raw materials for fiber and resin production with excellent heat resistance and mechanical strength. DMCD can not only be used as a modified material for polymers alone, but also has great uses in coatings. [0003] [0004] 1,4 Dimethyl cyclohexanedicarboxylate is prepared by catalytic hydrogenation of dimethyl terephthalate (DMT), using noble metal palladium catalysts, dimethyl terephthalate as raw material, low-pressure hydrogenation This produces dimethyl 1,4-cyclohexanedicarboxylate. The solvent is water or C1-C4 fatty alcohol or one of other solvents. The post-treatment pro...

Claims

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Application Information

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IPC IPC(8): C07C69/75C07C67/303
Inventor 邱志刚朱亮
Owner 江苏恒祥化学股份有限公司
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